CN103864097A - SAPO-34 molecular sieve adopting diglycol amine as template agent, and synthesis method thereof - Google Patents

SAPO-34 molecular sieve adopting diglycol amine as template agent, and synthesis method thereof Download PDF

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CN103864097A
CN103864097A CN201210535731.7A CN201210535731A CN103864097A CN 103864097 A CN103864097 A CN 103864097A CN 201210535731 A CN201210535731 A CN 201210535731A CN 103864097 A CN103864097 A CN 103864097A
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molecular sieve
sapo
dga
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silicon
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王德花
田鹏
刘中民
樊栋
张莹
苏雄
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China Ltd By Share Ltd New Technology (dalian) Limited By Share Ltd
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Abstract

The present invention provides a silicon-phosphorus-aluminum molecular sieve SAPO-34, which is characterized in that the anhydrous chemical composition is mDGA.(SixAlyPz)O2, wherein DGA is diglycol amine and is distributed in the molecular sieve cage and the pore channels, m is the number of moles of the diglycol amine template agent in per mole of (SixAlyPz)O2 and is 0.03-0.25, x, y and z respectively represent the mole fractions of Si, Al and P, x is 0.01-0.30, y is 0.40-0.60, z is 0.25-0.49, and (x+y+z) is equal to 1. The synthesized silicon-phosphorus-aluminum molecular sieve SAPO-34 can be adopted as the catalyst of the acid catalysis reaction such as the methanol-to-olefin reaction. The invention further relates to an application of the SAPO-34 molecular sieve in CH4 and CO2 absorption separation.

Description

A kind of SAPO-34 molecular sieve and synthetic method thereof taking diglycolamine as template
Technical field
The invention belongs to SAPO molecular sieve field, be specifically related to a kind of SAPO-34 molecular sieve and synthetic method thereof.
Background technology
Associating carbon company of the U.S. (UCC) researched and developed Novel phosphoric acid sial Series Molecules sieve (US4440871, US4499327)-SAPO-n molecular sieve in 1984, its be taking organic amine as template, taking hydrated aluminum oxide, phosphoric acid, silicon sol as aluminium source, He Gui source, phosphorus source, first obtain having organic amine/silicon aluminium phosphate complex body of microvoid structure by hydrothermal crystallization method, then remove by roasting that template (organic amine) obtains.Wherein, there is the aluminium silicophosphate molecular sieve SAPO-34 of CHA topological framework, due to its suitable pore passage structure, suitable protonic acid property, larger specific surface area, good absorption property and good thermostability and hydrothermal stability etc., make it in methanol-to-olefins (MTO) reaction, present excellent catalytic activity and selectivity.
SAPO-34 is Chabazite-type (CHA) molecular sieve, has and is piled up the octatomic ring elliposoidal cage and the three dimensional intersection pore passage structure that form by two six-rings according to ABC mode, and aperture is 0.38 × 0.38nm, belongs to small pore molecular sieve.Its space symmetr group is R3m, belongs to trigonal system (J.Phys.Chem., 1990,94:2730).SAPO-34 is made up of Si, Al, P and tetra-kinds of elements of O, and its composition can change within the specific limits, general n (Si) < n (P) < n (Al).
SAPO-34 molecular sieve generally adopts hydrothermal synthesis method, taking water as solvent, in enclosed high pressure still, carries out.What can be elected to be silicon source has silicon sol, active silica and a positive silicon ester, and there are activated alumina, pseudo-boehmite and aluminum alkoxide in aluminium source, and desirable Yu Lv source, silicon source is silicon sol and pseudo-boehmite; General 85% the phosphoric acid that adopts in phosphorus source.Conventional template comprises tetraethyl ammonium hydroxide (TEAOH), morpholine (MOR), piperidines (Piperidine), Isopropylamine (i-PrNH2), triethylamine (TEA), diethylamine (DEA), dipropyl amine etc. and their mixture.The selection of structure directing agent can produce certain influence for the microstructure of synthesis of molecular sieve, elementary composition and pattern, and and then affects its catalytic performance.
The present invention first taking diglycolamine as structure directing agent, under hydrothermal condition, synthesized pure phase SAPO-34 molecular sieve.The SAPO-34 molecular sieve of preparation shows good catalytic performance and gas adsorption separation performance in catalyzed reaction.
Summary of the invention
The object of the present invention is to provide a kind of SAPO-34 molecular sieve, this molecular sieve without hydrochemical compositions is: mDGA. (Si xal yp z) O 2, wherein: DGA is diglycolamine, be distributed in molecular sieve cage and duct; M is every mole of (Si xal yp z) O 2the mole number of middle diglycolamine, m=0.03~0.25; X, y, z represents respectively the molar fraction of Si, Al, P, and its scope is respectively x=0.01~0.30, y=0.40~0.60, z=0.25~0.49, and x+y+z=1; Preferable range is x=0.07~0.26, y=0.42~0.52, z=0.28~0.45, and x+y+z=1.The X-ray diffraction analysis of this molecular sieve has the diffraction peak shown in table 2.In its this molecular sieve X-ray diffraction analysis result, at least contain diffraction peak as shown in the table:
Figure BDA00002558239200021
Another object of the present invention is to provide a kind of synthetic method of SAPO-34 molecular sieve.
Another object of the present invention is to provide a kind of and synthesizes SAPO-34 molecular sieve and acid catalyzed reaction catalyzer prepared therefrom or oxygen-containing compound conversion to produce olefine catalysts by aforesaid method.
Another object of the present invention is to provide a kind of CH 4/ CO 2adsorption and separation material.
Technical problem to be solved by this invention is taking diglycolamine as structure directing agent, taking phosphorus source that conventional Zeolite synthesis was adopted, He Lv source, silicon source is as raw material, synthetic pure phase SAPO-34 molecular sieve under hydro-thermal or solvent thermal condition.
The invention is characterized in that preparation process is as follows:
A) deionized water, silicon source, aluminium source, phosphorus source and DGA are mixed according to a certain percentage, obtain having the initial gel mixture of following mole of proportioning:
SiO 2/Al 2O 3=0.05~2.5;
P 2O 5/Al 2O 3=0.5~1.5;
H 2O/Al 2O 3=5~200;
DGA/Al 2o 3=2.5~30; DGA is diglycolamine;
B) by step a) gained initial gel mixture pack Autoclaves for synthesis into, airtight, be warmed up to 150~220 DEG C, crystallization 5~72 hours under autogenous pressure;
C), after crystallization completes, solid product, through separating, to neutral, obtains described SAPO-34 molecular sieve after being dried with deionized water wash.
The silicon source of described step in a) is a kind of in silicon sol, active silica, positive silicon ester, metakaolin or several mixture arbitrarily; Aluminium source is a kind of or any several mixture in aluminium salt, activated alumina, aluminum alkoxide, metakaolin; Phosphorus source is a kind of or any several mixture in ortho-phosphoric acid, ammonium hydrogen phosphate, primary ammonium phosphate, Organophosphorous compounds or phosphorous oxides.
The crystallization process of step in b) can carry out in static state, also can dynamically carry out.
Described step is SiO in initial gel mixture a) 2/ Al 2o 3mol ratio preferably 0.15~2.0.
Described step is P in initial gel mixture a) 2o 5/ Al 2o 3mol ratio preferably 0.8~1.5.
Described step is H in initial gel mixture a) 2o/Al 2o 3mol ratio preferably 10~150.
Described step is DGA/Al in initial gel mixture a) 2o 3mol ratio preferably 5.5~16.
The invention still further relates to a kind of catalyzer of acid catalyzed reaction, it is that synthetic SAPO-34 molecular sieve roasting in 400~700 DEG C of air obtains by above-mentioned SAPO-34 molecular sieve or according to aforesaid method.
The catalyzer that the invention still further relates to a kind of oxygen-containing compound conversion to produce olefine reaction, it is that synthetic SAPO-34 molecular sieve roasting in 400~700 DEG C of air obtains by above-mentioned SAPO-34 molecular sieve or according to aforesaid method.
The invention still further relates to a kind of CH 4/ CO 2adsorption and separation material, it is that synthetic SAPO-34 molecular sieve roasting in 400~700 DEG C of air obtains by above-mentioned SAPO-34 molecular sieve or according to aforesaid method.
The beneficial effect that the present invention can produce comprises:
(1) obtain a kind of SAPO-34 molecular sieve taking diglycolamine as template.
(2) the SAPO-34 molecular sieve of preparing is to show good catalytic performance in low-carbon alkene reaction at methyl alcohol or dimethyl ether conversion.
(3) the SAPO-34 molecular sieve of preparing is at CH 4/ CO 2in fractionation by adsorption, show good selectivity.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of synthetic product in embodiment 1.
Embodiment:
The elementary composition Magix 2424X type ray fluorescence analysis instrument (XRF) that adopts Philips company is measured.
X-ray powder diffraction material phase analysis (XRD) adopts X ' the PertPRO X-ray diffractometer of Dutch PANalytical (PANalytical) company, Cu target, K α source of radiation (λ=0.15418nm), voltage 40KV, electric current 40mA.
SEM morphology analysis adopts the KYKY-AMRAY-1000B of Scientific Instrument Factory of C.A.S type scanning electronic microscope.
Nuclear magnetic resonance of carbon ( 13c MAS NMR) analyze the Infinity plus400WB solid state nmr wave spectrum analyzer that adopts Varian company of the U.S., with BBO MAS probe, magnetic manipulation field intensity is 9.4T.
The Vario EL Cube elemental analyser that CHN ultimate analysis adopts Germany to manufacture.
Below by embodiment in detail the present invention is described in detail, but the present invention is not limited to these embodiment.
Embodiment 1
Each feed molar proportion scale, crystallization condition and sample element set prejudice table 1.Concrete blending process is as follows, by 14g pseudo-boehmite (Al 2o 3quality percentage composition 72.5%) and 79.2g deionized water mix, then add 5.96g silicon sol (SiO 2quality percentage composition 30.24%), stir evenly the phosphoric acid (H of rear dropping 23.06g 3pO 4quality percentage composition 85%).31.5g diglycolamine (be called for short DGA, quality percentage composition 99%) is joined above in mixture, after stirring, gained gel is transferred in stainless steel cauldron.Mole proportioning of the each component of synthetic system is 3.0DGA: 0.30SiO 2: 1Al 2o 3: 1P 2o 5: 50H 2o.
Reactor is put into after baking oven to temperature programming to 200 DEG C dynamically lower crystallization 48h.After crystallization finishes, solid product is centrifugal, and washing, after drying, obtains former powder in 100 DEG C of air.Former powder sample does XRD test (table 2), and result shows that synthetic product has the feature of SAPO-34 structure.
The former powder sample of embodiment 1 is carried out to CHN ultimate analysis, CHN results of elemental analyses and XRF are measured to the inorganic elements composition normalization method obtaining, obtain the composition of molecular screen primary powder.
Table 1 Zeolite synthesis batching and crystallization condition table *
Figure BDA00002558239200051
Figure BDA00002558239200061
The XRD result of table 2 embodiment 1 sample
Embodiment 2-19
Concrete proportion scale and crystallization condition are in table 1, and concrete blending process is with embodiment 1.
Synthetic sample does XRD analysis, and data results and table 2 approach, and peak position is identical with shape, fluctuates in ± 10% scope according to the variation peak Relative Peak intensity of synthesis condition, shows that synthetic product has the feature of SAPO-34 structure.The elementary composition analysis of product the results are shown in Table 1.
Former powder sample to embodiment 1-10 carries out 13c MAS NMR analyzes, by with diglycolamine 13c MAS NMR standard spectrogram contrasts, and finds to only have in sample the resonance peak of diglycolamine.
Embodiment 20
The sample that embodiment 1 is obtained passes into air roasting 4 hours at 550 DEG C, then compressing tablet, be crushed to 20~40 orders.Take 5.0g sample and add the tank reactor that 30ml ethanol is housed, carry out ethanol dehydration reaction.Temperature of reaction is set in 150 DEG C, and reaction is carried out under whipped state.Reaction result demonstration, ethanol conversion can reach 92%, and in product, ether selectivity is 92%.
Embodiment 21
The sample that embodiment 1 is obtained passes into air roasting 4 hours at 550 DEG C, then compressing tablet, be crushed to 20~40 orders.Take 1.0g sample and pack fixed-bed reactor into, carry out MTO reaction evaluating.At 550 DEG C, logical nitrogen activation 1 hour, is then cooled to 450 DEG C and reacts.Methyl alcohol is carried by nitrogen, and nitrogen flow rate is 40ml/min, methyl alcohol weight space velocity 4.0h -1.Reaction product is analyzed (Varian3800, fid detector, capillary column PoraPLOTQ-HT) by online gas-chromatography.The results are shown in table 3.
The preparing olefin by conversion of methanol reaction result of table 3 sample
Embodiment 22
The sample that embodiment 10 is obtained passes into air roasting 4 hours at 550 DEG C.CO 2, CH 4adsorption isothermal line recorded by Micrometrics ASAP 2020 devices.Sample 350 DEG C of degassed pre-treatment 4 hours under vacuum state before measuring.Absorption test constant temperature is at 25 DEG C, and pressure is 101kpa.
The CO of table 4 sample 2/ CH 4fractionation by adsorption result
Figure BDA00002558239200082

Claims (9)

1. a SAPO-34 molecular sieve, is characterized in that, described molecular sieve without hydrochemical compositions is: mDGA (Si xal yp z) O 2represent, wherein: DGA is diglycolamine, m is every mole of (Si xal yp z) O 2the mole number of middle diglycolamine, m=0.03~0.25; X, y, z represents respectively the molar fraction of Si, Al, P, and its scope is respectively x=0.01~0.30, y=0.40~0.60, z=0.25~0.49, and x+y+z=1.
2. SAPO-34 molecular sieve according to claim 1, is characterized in that, X ray diffracting spectrum has diffraction peak with upper/lower positions:
No. 1 9.4445 2 15.942 3 17.7583 4 22.9708 5 29.428
3. a method for synthetic SAPO-34 molecular sieve claimed in claim 1, is characterized in that, synthesis step is as follows:
A) deionized water, silicon source, aluminium source, phosphorus source and DGA are mixed according to a certain percentage, obtain having the initial gel mixture of following mole of proportioning:
SiO 2/Al 2O 3=0.05~1.5;
P 2O 5/Al 2O 3=0.5~1.5;
H 2O/Al 2O 3=5~200;
DGA/Al 2o 3=2.5~30, DGA is diglycolamine;
B) by step a) gained initial gel mixture pack Autoclaves for synthesis into, airtight, be warmed up to 150~220 DEG C, crystallization 5~72 hours under autogenous pressure;
C), after crystallization completes, solid product, through separating, to neutral, obtains described SAPO-34 molecular sieve after being dried with deionized water wash.
4. in accordance with the method for claim 3, it is characterized in that, described step a) the silicon source in initial gel mixture is a kind of in silicon sol, active silica, positive silicon ester, metakaolin or several mixture arbitrarily; Aluminium source is a kind of or any several mixture in aluminium salt, activated alumina, aluminum alkoxide, metakaolin; Phosphorus source is a kind of or any several mixture in ortho-phosphoric acid, ammonium hydrogen phosphate, primary ammonium phosphate, Organophosphorous compounds or phosphorous oxides.
5. in accordance with the method for claim 3, it is characterized in that, the crystallization process of described step in b) static or dynamically under carry out.
6. in accordance with the method for claim 3, it is characterized in that, described step is DGA/Al in initial gel mixture a) 2o 3=5.5~16.
7. a catalyzer for acid catalyzed reaction, is characterized in that, according to the SAPO-34 molecular sieve described in claim 1-2 any one or according to either method described in claim 3-6, synthetic SAPO-34 molecular sieve roasting in 400~700 DEG C of air obtains.
8. the catalyzer of an oxygen-containing compound conversion to produce olefine reaction, it is characterized in that, according to the SAPO-34 molecular sieve described in claim 1-2 any one or according to either method described in claim 3-6, synthetic SAPO-34 molecular sieve roasting in 400~700 DEG C of air obtains.
9. a CH 4/ CO 2adsorption and separation material, is characterized in that, according to the SAPO-34 molecular sieve described in claim 1-2 any one or according to either method described in claim 3-6, synthetic SAPO-34 molecular sieve roasting in 400~700 DEG C of air obtains.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105366687A (en) * 2014-08-25 2016-03-02 中国科学院大连化学物理研究所 SAPO-34 molecular sieve with n-butylamine as template agent and synthetic method of SAPO-34 molecular sieve
CN111099637A (en) * 2018-10-25 2020-05-05 中国石油化工股份有限公司 Silicon-phosphorus-aluminum molecular sieve and preparation method thereof

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CN1087292A (en) * 1992-11-24 1994-06-01 中国科学院大连化学物理研究所 A kind of is the synthesized silicon phosphor aluminum molecular sieve and the preparation thereof of template with the triethylamine
CN1088483A (en) * 1992-12-19 1994-06-29 中国科学院大连化学物理研究所 A kind of is the synthesized silicon phosphor aluminum molecular sieve and the preparation thereof of template with the triethylamine
CN1096496A (en) * 1993-06-18 1994-12-21 中国科学院大连化学物理研究所 With the diethylamine is the template synthesized silicon-aluminum phosphate molecular sieve
CN1299776A (en) * 1999-12-15 2001-06-20 中国科学院大连化学物理研究所 Synthesis of silicon-aluminium phosphate molecular sieve with double or multiple template agent

Patent Citations (5)

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US4440871A (en) * 1982-07-26 1984-04-03 Union Carbide Corporation Crystalline silicoaluminophosphates
CN1087292A (en) * 1992-11-24 1994-06-01 中国科学院大连化学物理研究所 A kind of is the synthesized silicon phosphor aluminum molecular sieve and the preparation thereof of template with the triethylamine
CN1088483A (en) * 1992-12-19 1994-06-29 中国科学院大连化学物理研究所 A kind of is the synthesized silicon phosphor aluminum molecular sieve and the preparation thereof of template with the triethylamine
CN1096496A (en) * 1993-06-18 1994-12-21 中国科学院大连化学物理研究所 With the diethylamine is the template synthesized silicon-aluminum phosphate molecular sieve
CN1299776A (en) * 1999-12-15 2001-06-20 中国科学院大连化学物理研究所 Synthesis of silicon-aluminium phosphate molecular sieve with double or multiple template agent

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105366687A (en) * 2014-08-25 2016-03-02 中国科学院大连化学物理研究所 SAPO-34 molecular sieve with n-butylamine as template agent and synthetic method of SAPO-34 molecular sieve
CN105366687B (en) * 2014-08-25 2017-11-17 中国科学院大连化学物理研究所 A kind of molecular sieves of SAPO 34 and its synthetic method using n-butylamine as template
CN111099637A (en) * 2018-10-25 2020-05-05 中国石油化工股份有限公司 Silicon-phosphorus-aluminum molecular sieve and preparation method thereof
CN111099637B (en) * 2018-10-25 2023-03-03 中国石油化工股份有限公司 Silicon-phosphorus-aluminum molecular sieve and preparation method thereof

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